CN105385445B - A kind of method that co-dopant ions in Yttrium Tungstate base obtain white luminous fluorescent material - Google Patents
A kind of method that co-dopant ions in Yttrium Tungstate base obtain white luminous fluorescent material Download PDFInfo
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- CN105385445B CN105385445B CN201510727601.7A CN201510727601A CN105385445B CN 105385445 B CN105385445 B CN 105385445B CN 201510727601 A CN201510727601 A CN 201510727601A CN 105385445 B CN105385445 B CN 105385445B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7794—Vanadates; Chromates; Molybdates; Tungstates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
A kind of method that co-dopant ions in Yttrium Tungstate base obtain white luminous fluorescent material, it has five big steps：First, basis meets chemical formula：Y2‑x‑yWO6:xMn4+yEu3+Mol ratio weigh tungstic acid, yittrium oxide and europium oxide respectively as raw material；2nd, above-mentioned raw materials are put into agate mortar, and instill 1mL alcohol and help to grind, ground 30 minutes；3rd, the alumina crucible that said mixture is poured into 10mL is heated in Muffle furnace, and is heated to 1250 DEG C, 5 hours of Isothermal sinter with 3 DEG C/min heating rate；4th, cool to stopping Muffle furnace after less than 200 DEG C to power, room temperature is naturally cooled in stove；5th, the sample taken out after calcining is again placed in agate mortar, grinding makes it into fine powder shape, then sample is put into the sieve of 200 mesh progress sieving processing, that is, obtained different ions and adulterated under various concentrations the sample of Yttrium Tungstate.
Description
Technical field
The present invention provides a kind of method that co-dopant ions in Yttrium Tungstate base obtain white luminous fluorescent material, and it is red
The method of codope other elements in the luminous europium doping Yttrium Tungstate material of color.This method can change europium doping Yttrium Tungstate material
Glow color, regulate and control its color from feux rouges to white light.Belong to luminescent material technical field.
Background technology
20th century, the mankind also occurred in that environmental pollution while economic and scientific and technological high speed development, and energy shortage, ecology are broken
A series of significant problems such as bad.Wherein, energy problem is the task of top priority of the mankind.According to statistics, in China, resident's electric consumption on lighting is accounted for
According to 13% or so of Chinese generating total amount.The novel illumination apparatus of exploitation energy-conserving and environment-protective is a disaster of mankind's urgent need to resolve
Topic.White light-emitting diode, due to its efficiency high, long lifespan, response is fast, safety, the advantages of environmentally friendly, be described as after incandescent lamp,
After fluorescent lamp and high-intensity gas discharge lamp, " forth generation lighting source ".Its core is fluorescent material therein, so, find
A series of new phosphorses with premium properties with high conversion efficiency, high color rendering index (CRI) and safety non-toxic just become
One study hotspot of field of semiconductor illumination.
Tungstates is a kind of self-activation material, that is, does not need the participation of sensitizer or activator just to light.Near
Under ultraviolet, X-ray and cathode-ray exciting, they, which can show, efficiently lights, in intrinsic luminous covering visible light region
Very wide wave band, and luminescent spectrum is stable, is well suited as the host material of fluorescent material.This seminar utilizes high temperature solid-state
Method prepares monoclinic phase Yttrium Tungstate (Y2WO6) sample, it is found that it can launch yellow-green light under near ultraviolet excitation, it is excited
Spectrum has three absworption peaks, respectively in 280nm, 310nm and 340nm, charge transfer transition of the light sources between W-O, is
Y2WO6It is intrinsic luminous.
Doping refers to introduce external impurity in matrix, had a wide range of applications in illumination field.By in the substrate
The different elements of doping, relative to undoped with phase pure material, we can improve many properties of luminescent material, for example, adjusting
The glow color of material is controlled, its luminous intensity etc. is improved.Europium element (Eu) is a kind of conventional doping in semiconductor light emitting field
Element, exists as the form of activator in many matrix, in many matrix, can obtain new emission peak.In tungsten
In sour yttrium matrix, europium (Eu) also functions as the role of activator, and the Yttrium Tungstate for being doped with europium ion shows typical red hair
Light, is a kind of up-and-coming red fluorescence powder.The present invention is by the sample that europium adulterates, and codope enters manganese ion, manganese from
Son does not light wherein, as sensitizer, improves ratio of the sample intermediate waves length transmitting in all transmittings, makes sample blue
Move so that sample be converted to from emitting red light it is white luminous.The present invention has been widened obtains white luminous in Yttrium Tungstate base
Method, for instructing the research and development of new white fluorescent powder to be of great importance.
The content of the invention
1st, white luminous fluorescent material is obtained it is an object of the invention to provide a kind of co-dopant ions in Yttrium Tungstate base
Method.This method is easy, feasible, and it can significantly change the luminous color of Yttrium Tungstate material, obtains the sample of transmitting white light
Product.
2nd, technical solution of the invention：By manganese ion (Mn4+) and europium ion (Eu3+) codope enter Yttrium Tungstate base
In bottom, regulate and control europium-ion-doped (Eu3+) Yttrium Tungstate red fluorescence powder glow color, obtain white luminous fluorescent material.Specifically
Step is as follows：
Step one：According to meeting chemical formula：Y2-x-yWO6:xMn4+yEu3+Mol ratio weigh tungstic acid (WO respectively3,
Analysis it is pure, purity be 99.9%), yittrium oxide (Y2O3, analyze it is pure, purity be 99.9%), manganese oxide (MnO2, analyze pure, purity
97.5%) with europium oxide (Eu2O3, analyze pure, purity 99.9%) and it is used as raw material.
Step 2：The above-mentioned raw material weighed up is put into agate mortar, and instills 1mL alcohol and helps to grind, 30 points are ground
Clock, it is ensured that the full and uniform mixing of sample.
Step 3：In the alumina crucible that above-mentioned homogeneous mixture is poured into 10mL, and put it into Muffle furnace in sky
Heated in gas atmosphere, the temperature program(me) of heating is warm herein to be heated to 1250 DEG C from room temperature with about 3 DEG C/min heating rate
Spend lower 5 hours of Isothermal sinter.
Step 4：Stop Muffle furnace after being cooled to less than 200 DEG C to power, after annealing, make material naturally cold in stove
But room temperature is arrived.
Step 5：The sample of taking-up after calcining is again placed in agate mortar, grinding makes it into fine powder shape, then
Sample is put into the sieve of 200 mesh progress sieving processing, you can obtain different ions and adulterated under various concentrations Yttrium Tungstate
Sample.
3rd, it is an advantage of the invention that：By simply in doping europium ion (Eu3+) Yttrium Tungstate substrate in codope enter manganese
Ion (Mn4+), its glow color is regulated to white light from red, it is obtained in LEDphosphor for LED illumination and widely should
With.
Brief description of the drawings
Fig. 1：The emission spectrum schematic diagram of europium doping Yttrium Tungstate material.
Fig. 2：Europium, manganese are co-doped with the emission spectrum schematic diagram of Yttrium Tungstate material.
Fig. 3：The chromaticity coordinates figure of codope Yttrium Tungstate material.
Fig. 4：For FB(flow block) of the present invention.
Embodiment
With reference to embodiment and Fig. 1-Fig. 4, the present invention is described in detail, but the protection model of the present invention
Enclose and be not limited in the following example, the full content in application for patent should be included.
Embodiment 1
Step one：According to meeting chemical formula 0.02Mn0.02Eu：Y2WO6 mol ratio weighs the oxidations of 0.46368g tri- respectively
Tungsten, 0.44258g yittrium oxide, 0.0070g manganese oxide and 0.00323g europium oxides are used as raw material.
Step 2：The above-mentioned raw material weighed up is put into agate mortar, and instills 1mL essences and helps to grind, is ground 30 minutes,
Ensure the full and uniform mixing of sample.
Step 3：In the alumina crucible that above-mentioned homogeneous mixture is poured into 10mL, and put it into Muffle furnace in sky
Heated in gas atmosphere, the temperature program(me) of heating is warm herein to be heated to 1250 DEG C from room temperature with about 3 DEG C/min heating rate
Spend lower 5 hours of Isothermal sinter.
Step 4：Stop Muffle furnace after being cooled to less than 200 DEG C to power, after annealing, make material naturally cold in stove
But room temperature is arrived.
Step 5：The sample of taking-up after calcining is again placed in agate mortar, grinding makes it into fine powder shape, then
Sample is put into the sieve of 200 mesh progress sieving processing, you can obtain different ions and adulterated under various concentrations Yttrium Tungstate
Sample.
Embodiment 2
Step one：According to meeting chemical formula 0.01Mn0.02Eu：Y2WO6 mol ratio weighs the oxidations of 0.46368g tri- respectively
Tungsten, 0.43807g yittrium oxide, 0.00350g manganese dioxide and 0.00323g europium oxides are used as raw material.
Step 2：The above-mentioned raw material weighed up is put into agate mortar, and instills 1mL alcohol and helps to grind, 30 points are ground
Clock, it is ensured that the full and uniform mixing of sample.
Step 3：In the alumina crucible that above-mentioned homogeneous mixture is poured into 10mL, and put it into Muffle furnace in sky
Heated in gas atmosphere, the temperature program(me) of heating is warm herein to be heated to 1250 DEG C from room temperature with about 3 DEG C/min heating rate
Spend lower 5 hours of Isothermal sinter.
Step 4：Stop Muffle furnace after being cooled to less than 200 DEG C to power, after annealing, make material naturally cold in stove
But room temperature is arrived.
Step 5：The sample of taking-up after calcining is again placed in agate mortar, grinding makes it into fine powder shape, then
Sample is put into the sieve of 200 mesh progress sieving processing, you can obtain different ions and adulterated under various concentrations Yttrium Tungstate
Sample.
Claims (1)
1. a kind of method that co-dopant ions in Yttrium Tungstate base obtain white luminous fluorescent material, it is characterised in that：This method has
Body step is as follows：
Step one：According to meeting chemical formula：Y2-x-yWO6:xMn4+yEu3+Mol ratio weigh tungstic acid WO respectively3Analysis it is pure,
Purity is 99.9%, yittrium oxide Y2O3It is 99.9%, manganese dioxide MnO to analyze pure, purity2Analyze pure, purity 97.5% and oxidation
Europium Eu2O3Analyze pure, purity 99.9% and be used as raw material；
Step 2：The above-mentioned raw material weighed up is put into agate mortar, and instills 1mL alcohol and helps to grind, grinds 30 minutes, protects
Demonstrate,prove the full and uniform mixing of sample；
Step 3：In the alumina crucible that above-mentioned homogeneous mixture is poured into 10mL, and put it into Muffle furnace in air gas
Heated in atmosphere, the temperature program(me) of heating is to be heated to 1250 DEG C from room temperature with 3 DEG C/min heating rate, at this temperature constant temperature
Sinter 5 hours；
Step 4：Stop Muffle furnace after being cooled to less than 200 DEG C to power, after annealing, allow material to be naturally cooled in stove
Room temperature；
Step 5：The sample of taking-up after calcining is again placed in agate mortar, grinding makes it into fine powder shape, then sample
Product are put into the sieve of 200 mesh progress sieving processing, that is, obtain different ions and adulterated under various concentrations the sample of Yttrium Tungstate；
Wherein, x=0.02 or 0.01, y=0.02.
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| DE10036940A1 (en) * | 2000-07-28 | 2002-02-07 | Patent Treuhand Ges Fuer Elektrische Gluehlampen Mbh | Luminescence conversion LED |
| CN1239673C (en) * | 2003-10-23 | 2006-02-01 | 北京有色金属研究总院 | Red luminescent powder in use for LED, preparing method and electric light source produced |
| US7573072B2 (en) * | 2004-03-10 | 2009-08-11 | Lumination Llc | Phosphor and blends thereof for use in LEDs |
| CN100412157C (en) * | 2006-06-09 | 2008-08-20 | 中国科学院上海硅酸盐研究所 | X-ray excited rare-earth ion blended tungstate flash luminous material and its preparing method |
| CN100540629C (en) * | 2007-11-12 | 2009-09-16 | 中国科学院长春光学精密机械与物理研究所 | Near ultraviolet or blue-light excited red fluorescence powder and preparation method thereof |
| CN101255337B (en) * | 2008-03-13 | 2010-06-09 | 同济大学 | Preparation method of red-light fluorescent powder for LED or PDP display |
| CN102417815A (en) * | 2011-09-01 | 2012-04-18 | 上海师范大学 | Rare earth tungstate phosphor matrix, its preparation method and application |
| CN104085928B (en) * | 2014-07-17 | 2016-04-13 | 中国科学院上海硅酸盐研究所 | Rare earth ion doped tungstate flash film and preparation method thereof |
| CN104194786B (en) * | 2014-07-29 | 2016-03-02 | 北京航空航天大学 | A kind of in Yttrium Tungstate material dopant ion improve the method for its luminescent properties |
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